Sample table for high-pressure in-situ X-ray diffraction test
By designing a sample stage suitable for X-ray diffractometers, the problem of high-pressure in-situ X-ray diffraction testing that cannot be performed in existing technologies has been solved, enabling efficient fine-tuning and testing of samples and expanding the application range of X-ray diffractometers.
Patent Information
- Application Number
- CN202520288579.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-21
- Publication Date
- 2025-12-09
- Estimated Expiration
- 2035-02-21
AI Technical Summary
Existing X-ray diffractometers cannot perform high-pressure (≤50GPa) in-situ X-ray diffraction tests, mainly due to the lack of a sample stage specifically designed to support diamond anvil cells.
A sample stage for high-pressure in-situ X-ray diffraction testing was designed, comprising a diamond anvil retaining ring, a multi-vector displacement stage, and a sample holder base. The multi-vector displacement design can fix the diamond anvil and make fine adjustments up and down, left and right, and forward and backward, making it compatible with X-ray diffractometers.
It enables high-pressure in-situ X-ray diffraction testing, expands the characterization capabilities of X-ray diffractometers, overcomes the problem of excessive weight of diamond anvil cells, and provides a function for fine-tuning the optimal position of the sample.
Smart Images
Figure CN223650481U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the technical field of crystal measurement devices, specifically relating to a sample stage for high-pressure in-situ X-ray diffraction testing. Background Technology
[0002] X-ray diffraction is a technique that uses the diffraction effect of X-rays in crystalline materials to analyze their structure. High-pressure in-situ X-ray diffraction can observe the changes in material structure with pressure, helping to reveal the nature of these structural changes.
[0003] In the existing technology, the press used for high-pressure in-situ X-ray diffraction testing is a diamond anvil cell (DAC), which is relatively heavy compared to ordinary samples. Currently, there is no sample stage specifically designed to support the diamond anvil cell in X-ray diffractometers on the market, which makes it impossible for some X-ray diffractometers to perform high-pressure (≤50GPa) in-situ X-ray diffraction testing. Utility Model Content
[0004] To address the problem that conventional X-ray diffractometers in the prior art cannot perform high-pressure in-situ X-ray diffraction testing, this invention provides a sample stage for high-pressure in-situ X-ray diffraction testing. This sample stage can fix a diamond anvil cell (DAC), is compatible with an X-ray diffractometer, and allows for fine-tuning of the sample position in the up-down, left-right, and front-back directions, so as to facilitate high-pressure (≤50GPa) in-situ X-ray diffraction testing.
[0005] This utility model is achieved through the following technical solution:
[0006] A sample stage for high-pressure in-situ X-ray diffraction testing includes, from top to bottom, a diamond anvil retaining ring 1, a multi-vector displacement stage 2, and a sample holder base 3 connected in sequence. The diamond anvil retaining ring 1 is used to fix the diamond anvil. The multi-vector displacement stage 2 includes, from top to bottom, a vertical displacement plate 21, a horizontal displacement plate 22, a front-back displacement plate 24, and a multi-vector displacement stage base 25 connected in sequence. The vertical displacement plate 21 is used to realize the vertical movement of the multi-vector displacement stage 2, the horizontal displacement plate 22 is used to realize the horizontal movement of the multi-vector displacement stage 2, and the front-back displacement plate 24 is used to realize the front-back movement of the multi-vector displacement stage 2. The multi-vector displacement stage base 25 is connected to the sample holder base 3, and the sample holder base 3 is fixed in the X-ray diffractometer by nuts for characterization testing.
[0007] Furthermore, the diamond anvil fixing ring 1 includes a diamond anvil locking plate 10, a diamond anvil locking screw 11, and a diamond anvil base 12; one end of the diamond anvil base 12 is connected to the diamond anvil locking plate 10 through the diamond anvil locking screw 11, and the other end is connected to the upper and lower displacement plates 21 of the multi-vector displacement stage 2.
[0008] Furthermore, the upper end of the diamond anvil base 12 and the diamond anvil locking piece 10 are both semi-circular, and the circle formed after the connection is similar to the shape of the diamond anvil, and is locked by the diamond anvil locking screw 11; the lower end of the diamond anvil base 12 is a cuboid plane, which is used to connect with the upper and lower displacement plates 21 of the multi-vector displacement stage 2.
[0009] Furthermore, the vertical displacement plate 21 and the horizontal displacement plate 22 are connected by a vertical displacement rotating screw 20; the lower end face of the vertical displacement plate 21 is provided with a vertical displacement plate buckle 27, and the upper end face of the horizontal displacement plate 22 is provided with a vertical displacement plate buckle groove 28. The vertical displacement plate buckle groove 28 is used to place the vertical displacement plate buckle 27 for limiting the position. By rotating the vertical displacement rotating screw 20, the vertical displacement plate 21 can be moved up or down. The vertical displacement plate buckle 27 and the vertical displacement plate buckle groove 28 can ensure that the displacement plate 21 does not tilt during the vertical movement.
[0010] Furthermore, the left and right displacement plate 22 and the front and rear displacement plate 24 are connected by left and right displacement rotating screws 23; the lower end face of the left and right displacement plate 22 is provided with a transverse wedge block, and the upper end face of the front and rear displacement plate 24 is provided with a transverse wedge groove. The transverse wedge block can move left and right in the transverse wedge groove, and rotating the left and right displacement rotating screws 23 can make the left and right displacement plate 22 move to the left or right.
[0011] Furthermore, the front and rear displacement plate 24 is connected to the multi-vector displacement stage base 25 by a front and rear displacement rotating screw 26; the lower end face of the front and rear displacement plate 24 is provided with a vertical wedge block, and the upper end face of the multi-vector displacement stage base 25 is provided with a vertical wedge groove. The vertical wedge block can move back and forth in the vertical wedge groove, and rotating the front and rear displacement rotating screw 26 can make the front and rear displacement plate 24 move forward or backward.
[0012] Compared with the prior art, the advantages of this utility model are as follows:
[0013] This invention discloses a sample stage for high-pressure in-situ X-ray diffraction testing. A locking ring secures the diamond anvil cell (DAC), allowing it to be mounted within the X-ray diffractometer, overcoming the problem of excessive weight associated with DACs. More importantly, the multi-vector displacement design allows for fine-tuning of the sample, enabling it to be moved to the optimal position for high-pressure in-situ X-ray diffraction testing. This invention expands the characterization capabilities of X-ray diffractometers and has promising application prospects. Attached Figure Description
[0014] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. In all the drawings, similar elements or parts are generally identified by similar reference numerals. In the drawings, the elements or parts are not necessarily drawn to scale.
[0015] Figure 1 This is a schematic diagram of a sample stage used for high-pressure in-situ X-ray diffraction testing.
[0016] Figure 2 This is a schematic diagram of the split structure of a sample stage for high-pressure in-situ X-ray diffraction testing.
[0017] Figure 3 This is a schematic diagram of a sample stage used for high-pressure in-situ X-ray diffraction testing.
[0018] In the figure: 1. Diamond anvil fixing ring; 2. Multi-vector displacement stage; 3. Sample holder base; 4. Diamond anvil; 5. X-ray; 6. Diffraction ring.
[0019] 10. Diamond anvil locking plate; 11. Diamond anvil locking screw; 12. Diamond anvil base;
[0020] 20. Up and down displacement rotating screw, 21. Up and down displacement plate, 22. Left and right displacement plate, 23. Left and right displacement rotating screw, 24. Front and rear displacement plate, 25. Multi-vector displacement stage base, 26. Front and rear displacement rotating screw, 27. Up and down displacement plate buckle, 28. Up and down displacement plate buckle groove. Detailed Implementation
[0021] To clearly and completely describe the technical solution and its specific working process of this utility model, the specific embodiments of this utility model are as follows, in conjunction with the accompanying drawings:
[0022] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.
[0023] Example 1
[0024] like Figure 1 and Figure 2As shown, this embodiment provides a sample stage for high-pressure in-situ X-ray diffraction testing, comprising, from top to bottom, a diamond anvil fixing ring 1, a multi-vector displacement stage 2, and a sample holder base 3 connected in sequence. The diamond anvil fixing ring 1 is used to fix the diamond anvil. The multi-vector displacement stage 2 comprises, from top to bottom, a vertical displacement plate 21, a horizontal displacement plate 22, a front-back displacement plate 24, and a multi-vector displacement stage base 25 connected in sequence. The vertical displacement plate 21 is used to realize the vertical movement of the multi-vector displacement stage 2, the horizontal displacement plate 22 is used to realize the horizontal movement of the multi-vector displacement stage 2, and the front-back displacement plate 24 is used to realize the front-back movement of the multi-vector displacement stage 2. The multi-vector displacement stage base 25 is connected to the sample holder base 3, and the sample holder base 3 is fixed in the X-ray diffractometer by nuts for characterization testing.
[0025] In this embodiment, the diamond anvil fixing ring 1 includes a diamond anvil locking plate 10, a diamond anvil locking screw 11, and a diamond anvil base 12; one end of the diamond anvil base 12 is connected to the diamond anvil locking plate 10 through the diamond anvil locking screw 11, and the other end is connected to the upper and lower displacement plates 21 of the multi-vector displacement stage 2.
[0026] In this embodiment, the upper end of the diamond anvil base 12 and the diamond anvil locking piece 10 are both semi-circular. After being connected, the circle formed is similar in shape to the diamond anvil and is locked by the diamond anvil locking screw 11. The lower end of the diamond anvil base 12 is a cuboid plane, which is used to connect with the upper and lower displacement plates 21 of the multi-vector displacement stage 2.
[0027] In this embodiment, the vertical displacement plate 21 and the horizontal displacement plate 22 are connected by a vertical displacement rotating screw 20. The lower end face of the vertical displacement plate 21 is provided with a vertical displacement plate buckle 27, and the upper end face of the horizontal displacement plate 22 is provided with a vertical displacement plate buckle groove 28. The vertical displacement plate buckle groove 28 is used to place the vertical displacement plate buckle 27 for limiting the position. By rotating the vertical displacement rotating screw 20, the vertical displacement plate 21 can be moved up or down. The vertical displacement plate buckle 27 and the vertical displacement plate buckle groove 28 can ensure that the displacement plate 21 does not tilt during the vertical movement.
[0028] The vertical displacement rotating screw 20 passes through the vertical displacement plate 21. When the vertical displacement rotating screw 20 is rotated, the vertical displacement rotating screw 20 pushes against the left and right displacement plates 22 to lift the vertical displacement plate 21, thereby realizing vertical movement.
[0029] In this embodiment, the left and right displacement plate 22 and the front and rear displacement plate 24 are connected by left and right displacement rotating screws 23; the lower end face of the left and right displacement plate 22 is provided with a transverse wedge block, and the upper end face of the front and rear displacement plate 24 is provided with a transverse wedge groove. The transverse wedge block can move left and right in the transverse wedge groove, and rotating the left and right displacement rotating screws 23 can make the left and right displacement plate 22 move to the left or right.
[0030] The left and right displacement plate 22, the front and rear displacement plate 24, and the multi-vector displacement stage base 25 each have half of the screw hole in contact with the screw. The threads of the upper and lower screw holes of the same screw are opposite. Taking the left and right displacement rotating screw 23 as an example, the thread of the left and right displacement rotating screw 23 is parallel, the screw hole thread on the lower front and rear displacement plate 24 is also parallel, and the thread on the left and right displacement plate 22 is oblique. When the left and right displacement rotating screw 23 is rotated, the front and rear displacement plate 2 does not move, thereby realizing the left and right movement of the left and right displacement plate 22. The same applies to the front and rear movement.
[0031] In this embodiment, the front and rear displacement plate 24 is connected to the multi-vector displacement stage base 25 by a front and rear displacement rotating screw 26; the lower end face of the front and rear displacement plate 24 is provided with a vertical wedge block, and the upper end face of the multi-vector displacement stage base 25 is provided with a vertical wedge groove. The vertical wedge block can move back and forth in the vertical wedge groove, and rotating the front and rear displacement rotating screw 26 causes the front and rear displacement plate 24 to move forward or backward.
[0032] like Figure 3 The diagram shown is a schematic representation of the combined operation of a sample stage and an X-ray diffractometer for high-pressure in-situ X-ray diffraction testing according to this embodiment. The working process of the sample stage is as follows:
[0033] First, place the calibrated pressure diamond anvil 4 on the diamond anvil base 12, add the diamond anvil locking piece 10, and rotate the diamond anvil locking screw 11 to fix the diamond anvil 4.
[0034] Next, place the sample stage of this embodiment in the sample testing area of the X-ray diffractometer, and rotate the nut of the sample holder base 3 to fix the sample stage in the X-ray diffractometer.
[0035] Next, rotate the vertical displacement screw 20 to move the sample in the diamond anvil 4 vertically until it reaches the middle position of the CCD screen; rotate the horizontal displacement screw 23 to move the sample in the diamond anvil 4 horizontally and vertically until it reaches the middle position of the CCD screen; rotate the forward and backward displacement screw 26 to move the sample in the diamond anvil 4 forward and backward until the clearest image is seen on the CCD screen.
[0036] Next, close the X-ray diffractometer door, open the X-ray diffractometer shield, expose the sample for 30 minutes, and collect diffraction ring information.
[0037] Finally, after the signal collection is complete, open the X-ray diffractometer chamber door, take out the high-pressure in-situ X-ray diffraction test sample stage, rotate the diamond anvil locking screw 11 to remove the diamond anvil 4, rotate the diamond anvil 4 screw to apply pressure to the sample, and repeat the above four steps to conduct a new round of testing.
[0038] The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited to the specific details of the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.
[0039] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable way without contradiction. In order to avoid unnecessary repetition, this utility model will not describe the various possible combinations separately.
[0040] Furthermore, various different embodiments of this utility model can be combined in any way, as long as they do not violate the spirit of this utility model, they should also be regarded as the content disclosed by this utility model.
Claims
1. A sample stage for high-pressure in-situ X-ray diffraction testing, characterized in that, From top to bottom, it includes a diamond anvil fixing ring (1), a multi-vector displacement stage (2), and a sample holder base (3) connected in sequence. The diamond anvil fixing ring (1) is used to fix the diamond anvil. The multi-vector displacement stage (2) includes, from top to bottom, a vertical displacement plate (21), a horizontal displacement plate (22), a front-back displacement plate (24), and a multi-vector displacement stage base (25) connected in sequence. The vertical displacement plate (21) is used to realize the vertical movement of the multi-vector displacement stage (2). The horizontal displacement plate (22) is used to realize the horizontal movement of the multi-vector displacement stage (2). The front-back displacement plate (24) is used to realize the front-back movement of the multi-vector displacement stage (2). The multi-vector displacement stage base (25) is connected to the sample holder base (3). The sample holder base (3) is fixed in the X-ray diffractometer by a nut for characterization testing.
2. The sample stage for high-pressure in-situ X-ray diffraction testing as described in claim 1, characterized in that, The diamond anvil fixing ring (1) includes a diamond anvil locking plate (10), a diamond anvil locking screw (11), and a diamond anvil base (12); one end of the diamond anvil base (12) is connected to the diamond anvil locking plate (10) through the diamond anvil locking screw (11), and the other end is connected to the upper and lower displacement plates (21) of the multi-vector displacement stage (2).
3. A sample stage for high-pressure in-situ X-ray diffraction testing as described in claim 2, characterized in that, The upper end of the diamond anvil base (12) and the diamond anvil locking plate (10) are both semi-circular. After they are connected, the circle formed is similar to the shape of the diamond anvil and is locked by the diamond anvil locking screw (11). The lower end of the diamond anvil base (12) is a cuboid plane, which is used to connect with the upper and lower displacement plates (21) of the multi-vector displacement stage (2).
4. The sample stage for high-pressure in-situ X-ray diffraction testing as described in claim 1, characterized in that, The upper and lower displacement plates (21) and the left and right displacement plates (22) are connected by upper and lower displacement rotating screws (20); the lower end face of the upper and lower displacement plates (21) is provided with upper and lower displacement plate buckles (27), and the upper end face of the left and right displacement plates (22) is provided with upper and lower displacement plate buckle grooves (28). The upper and lower displacement plate buckle grooves (28) are used to place the upper and lower displacement plate buckles (27) for limiting the movement. By rotating the upper and lower displacement rotating screws (20), the upper and lower displacement plates (21) can be moved up or down. The upper and lower displacement plate buckles (27) and the upper and lower displacement plate buckle grooves (28) can ensure that the displacement plates (21) do not tilt during the up and down movement.
5. A sample stage for high-pressure in-situ X-ray diffraction testing as described in claim 1, characterized in that, The left and right displacement plates (22) and the front and rear displacement plates (24) are connected by left and right displacement rotating screws (23); the lower end face of the left and right displacement plates (22) is provided with a transverse wedge block, and the upper end face of the front and rear displacement plates (24) is provided with a transverse wedge groove. The transverse wedge block can move left and right in the transverse wedge groove. Rotating the left and right displacement rotating screws (23) causes the left and right displacement plates (22) to move to the left or right.
6. A sample stage for high-pressure in-situ X-ray diffraction testing as described in claim 1, characterized in that, The front and rear displacement plate (24) is connected to the multi-vector displacement stage base (25) by a front and rear displacement rotating screw (26); the lower end face of the front and rear displacement plate (24) is provided with a vertical wedge block, and the upper end face of the multi-vector displacement stage base (25) is provided with a vertical wedge groove. The vertical wedge block can move back and forth in the vertical wedge groove. Rotating the front and rear displacement rotating screw (26) causes the front and rear displacement plate (24) to move forward or backward.